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ABSTRACT

LIQUID, RANDOM ETHYLENE/C3-C20 A-OLEFIN COPOLYMERS HAVING AN AVERAGE HYDROXYL FUNCTIONALLY OF ABOUT 1.8-3.0 AND A NUMBER-AVERAGE MOLECULAR WEIGHT OF ABOUT 3003500, USEFUL AS STARTING MATERIALS FOR THE PREPARATION OF HIGH MOLECULAR WEIGHT POLYURETHANES AND POLYESTERS, ARE MADE FROM RANDOM ETHYLENE/C3-C20 A-OLEFIN COPOLYMERS (HAVING ABOUT 1.8-3.0 CARBOXYLIC GROUPS, 1, 0-1.5 CHAIN ESTER GROUPS, 0,4-1 CHAIN KETONE GROUPS, AND 1.0-2.0 CHAIN HYDROXYL GROUPS PER MOLECULE ON THE AVERAGE) BY A PROCESS INVOLVING THE FOLLOWING CONSECUTIVE STEPS: (1) TREATING THE CARBOXYL-CONTAINING COPOLYMER AT ABOUT 20*C. TO ABOUT 100*C. IN AN INERT SOLVENT WITH ABOUT 5-10 MOLES EACH OF PCL2 AND PCL5 PER MOLE OF POLYMER TO CONVERT SUBSTANTIALLY ALL HYDROXYL GROUPS TO CHLORIDE AND CARBONYL GROUPS OF GEM-DICHLORIDE, (2) REMOVING EXCESS PHOSPHORUS CHLORIDES, (3) CONTACTING THE POLYMERIC PRODUCT OF (1) IN AN INERT DRY SOLVENT (PREFERABLY TETRAHYDROFURAN) WITH ABOUT 3-6 MOLES OF LIA)&#39;&#39;4 AND 10-60 MOLES OF LIH PER MOLE OF POLYMER TO REDUCE SUBSTANTIALLY ALL CARBOXYL, CARBOXYLIC ACID CHLORIDE, AND ESTER GROUPS TO HYDROXYL GROUPS AND ALL GEM-DICHLORIDE GROUPS TO METHYLENE GROUPS, AND (4) DECOMPOSING THE UNCHANGED METAL HYDRIDE WITH WATER OR ALCOHOL (PREFERABLY IN THE PRESENCE OF IONS OF A NEUTRAL METAL SALT SUCH AS NACL) AND RECOVERING THE HYDROXYL-SUBSTITUTED POLYMER.

"-1 "*1" "r; l a" "we "1T": "*2 DEFENbll/E EUR lluol llltljls UNITED STATES PATEYT AND TRADE? Published at the request of the applied t or own-:1 in accordance with the *Tciico of 5320. 1C, 18Gb, 863 0G. CS7. The abstracts of Defensive Publication iplicaticns are identified by 'lnctl n1 r god chronologically. The heading of each abstract indicates the lllll.lll!ll o T l .awing's contained in the application as originally tiled. The ill-es of t ction and reproduction may be purchased for 30 cents a sheet.

has) op um tions are t Defensive Publication applications have not been mined. to the m Trademark Otfice makes no assertion as to the novelty cl t c disclosed subject mutt PUBLISHED JULY 1, 1975 31 36 081 NOVEL HYDRDXYL-TERMLJAETJD FQLYMLERS Robin Nikolas Greene, 4, M25 Run E lond, New Albany, ind. 57 1213 Filed Mar. 12, 197 Ser. No 4:30,.557 int. Cl. 69% 31/18 US. Cl. 268 635 R No Drawing. l6 Specil tion Liquid, random ethylene/C -C a-oleiln copolynicrs having an average hydroxyl functionality of about 1.8-3.0 and a number-average molecular Weight of about 300- 350-0, useful as starting materials for the preparation of high molecular Weight polyurethanes and polyesters, are made from random ethyIenc/C 'C tit-olefin copolymcrs (having about 1.8-3.0 carboxylic groups, 1.04.5 chain ester groups, 0.4l chain ketone groups, and l.02.0 chain hydroxyl groups per molecule on the average) by a process involving the following consecutive steps:

(1) treating the carboxyl-containing copolymer at about 20 C. to about 100 C. in an inert solvent with about 5-10 moles each of PCl and PCi per mole of polymer to convert substantially all hydroxyl groups to chloride and carbonyl groups to gem-dichloride;

(2) removing excess phosphorus chlorides;

(3) contacting the polymeric product of (1) in an inert dry solvent (preferably tctrahydrot'uran) with about 3-6 moles of LiAll-L; and l060 moles of Lil-l per mole of polymer to reduce substantially all carbonyl, carboxylic acid chloride, and ester groups to hydroxyl groups and all gem-dichloride groups to methylene groups; and

(4) decomposing the unchanged metal hydridcs with water or alcohol (preferably in the presence of ions of a neutral metal salt such as NaCl) and recovering the hydroXyl-substitutcd polymer.

of alleged invention. The Patent and 

